CN114147216B - Method for adding low-boiling-point easily-oxidized metal elements into steel product and printing device - Google Patents

Method for adding low-boiling-point easily-oxidized metal elements into steel product and printing device Download PDF

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CN114147216B
CN114147216B CN202111165822.1A CN202111165822A CN114147216B CN 114147216 B CN114147216 B CN 114147216B CN 202111165822 A CN202111165822 A CN 202111165822A CN 114147216 B CN114147216 B CN 114147216B
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powder
steel
low
boiling
point easily
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CN114147216A (en
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林腾昌
杨勇
苏杰
王长军
李龙飞
孟利
宁静
刘赓
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Central Iron and Steel Research Institute
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/70—Recycling
    • B22F10/73—Recycling of powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y30/00—Apparatus for additive manufacturing; Details thereof or accessories therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10—Pre-treatment
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

The invention relates to a method for adding low-boiling-point easily-oxidized metal elements into a steel product and a printing device, belonging to the field of additive manufacturing. The problem that the oxygen content of steel powder is too high in the prior art, and the performance of a printed piece is finally affected is solved. A method for adding low-boiling-point easily-oxidized metal elements into a steel product comprises the steps of taking steel powder and low-boiling-point easily-oxidized metal powder as raw materials, carrying out particle size screening, drying and powder mixing under a protective atmosphere, and carrying out additive manufacturing and printing after powder laying. The method realizes the reduction of the oxygen content in the steel product, changes the existence form of the oxide inclusion, and finally improves the performance of the special steel printing piece, wherein the steel product contains high-content low-boiling-point easily-oxidized metal elements.

Description

Method for adding low-boiling-point easily-oxidized metal elements into steel product and printing device
Technical Field
The invention belongs to the field of additive manufacturing, and particularly relates to a method for adding low-boiling-point easily-oxidizable metal elements into a steel product and a special steel powder and low-boiling-point easily-oxidizable metal powder mixing and printing device.
Background
The additive manufacturing metal powder is an important part of the metal part additive manufacturing industry chain, and the metal powder for additive manufacturing is mainly focused on titanium alloy, high-temperature alloy, cobalt-chromium alloy, special steel and other materials at present.
The special steel base material of the special steel powder for additive manufacturing is generally obtained by smelting through the traditional processes of vacuum metallurgy, electroslag metallurgy and the like, and then qualified special steel powder is obtained through four methods of a plasma rotating electrode method (PREP), a plasma atomization method (PA), a GAs atomization method (GA) and a plasma spheroidization method (PS). After the special steel base metal (the oxygen content is less than or equal to 20 ppm) is prepared into the special steel powder (the diameter is dozens of microns), the oxygen content of the special steel powder is suddenly increased (the oxygen content is 100-400 ppm) because the specific surface area of the powder is large and the powder is easy to adsorb oxygen in the protective atmosphere.
In order to meet the requirements of additive manufacturing equipment and process, the metal powder has to have the characteristics of low oxygen content, good sphericity, narrow particle size distribution interval, high apparent density and the like. When the metal powder with high oxygen content is used for manufacturing and printing special steel pieces in an additive mode, oxygen is easy to combine with alloy elements of the special steel to form inclusions, so that the oxygen content of the printed pieces is high (the oxygen content is larger than or equal to 60 ppm), and the performance of the printed pieces is influenced finally.
Furthermore, in special steel products, low-boiling, easily oxidizable metallic elements are generally added during the metallurgical process. In the traditional metallurgical processes such as vacuum metallurgy, electroslag metallurgy and the like, a molten pool is about 1600 ℃ for a long time when special steel is smelted, low-boiling-point easily-oxidizable metal elements are difficult to add in the smelting process, and the low-boiling-point easily-oxidizable metal is easy to react with oxygen to generate complex oxidized inclusions, so that the performance of a product is influenced.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a method for adding low-boiling point easily-oxidizable metal element to a steel product, and a mixed printing device for steel powder and low-boiling point easily-oxidizable metal powder, so as to solve one of the following technical problems: (1) The problem of overhigh oxygen content in the printed piece manufactured by the special steel powder additive in the prior art is solved, so that the beneficial effect of improving the performance of the printed piece is achieved; (2) It is difficult to add high content of low boiling point easily oxidizable metallic elements to steel products.
The invention is mainly realized by the following technical scheme:
on one hand, the invention provides a method for adding low-boiling point easily-oxidizable metal elements into a steel product, which comprises the steps of taking steel powder and low-boiling point easily-oxidizable metal powder as raw materials, carrying out particle size screening, drying and powder mixing under a protective atmosphere, and carrying out additive manufacturing printing after powder spreading.
Further, the steel powder is special steel powder, the special steel powder is obtained by smelting through a metallurgical process, and then the steel powder for additive manufacturing is obtained through a plasma rotating electrode method, a plasma atomization method, an air atomization method or a plasma spheroidization method.
Further, the method comprises the following steps:
step 1: respectively screening the steel powder and the low-boiling point easily-oxidized metal powder in granularity under a protective atmosphere and sealing for later use;
step 2: drying the steel powder and the low-boiling point easily-oxidized metal powder under a protective atmosphere, cooling to room temperature, and then filling the steel powder and the low-boiling point easily-oxidized metal powder into a steel powder bin and a low-boiling point easily-oxidized metal powder bin for later use;
and 3, step 3: accurately controlling the weight of the steel powder and the low-boiling point easily-oxidized metal powder to be fed into a powder mixing bin;
and 4, step 4: uniformly mixing the powder;
and 5: powder spreading, additive manufacturing printing, realize the addition of low boiling point easily-oxidized metal elements in the steel product.
Further, the weight M of the low-boiling point easily-oxidized metal powder Boiling water With the weight M of steel powder Steel Satisfy the relation:
a＝M boiling water /(M Boiling water +M Steel ) Wherein a is more than 25 times of the oxygen content of the steel powder.
Further, in the step 1, when the additive manufacturing printing is performed by adopting a laser printer, the particle sizes of the steel powder and the low-boiling point easily-oxidized metal powder are 15-53 μm; when the additive manufacturing printing is carried out by adopting a plasma beam printer, the granularity of the steel powder and the low-boiling point easily-oxidized metal powder is 53-105 mu m.
Further, in step 2, the protective atmosphere is argon.
Further, in the step 2, argon is introduced into the vacuum baking oven for 5-10 min, the sealing bag filled with the steel powder and the low-boiling point easily-oxidizable metal powder is opened in an argon environment, the steel powder and the low-boiling point easily-oxidizable metal powder are flatly laid in different baking trays, and the baking is carried out under the condition that the vacuum degree is less than or equal to 100 Pa.
Further, in the step 2, the drying temperature is 100-200 ℃, and the drying time is 4-8 h.
Furthermore, in the step 3, the blanking proportion m of the low-boiling-point easily-oxidized metal powder and the special steel powder Boiling powder /m Powder under steel And M Boiling water /M Steel The difference is less than or equal to 0.01 percent.
On the other hand, the invention also provides a special steel powder and low-boiling-point easily-oxidized metal powder mixing and printing device which is used for realizing the method and comprises a powder bin, a powder mixing bin (5), a powder storage bin (6) and a shielding gas unit which are sequentially connected;
the powder bin comprises a special steel powder bin and a low-boiling point easily-oxidized metal powder bin which are respectively and independently communicated with the powder mixing bin, and regulating valves are arranged on connecting pipelines of the powder bin and the powder mixing bin;
the powder bin and the powder mixing bin are independent and closed devices and are provided with gas inlets, and the gas inlets are connected with the shielding gas unit.
Compared with the prior art, the invention can at least realize one of the following technical effects:
(1) The invention provides a method for adding low-boiling-point easily-oxidizable metal elements into a steel product, which directly adopts steel powder and low-boiling-point easily-oxidizable metal powder as raw materials, performs particle size screening, drying and powder mixing under a protective atmosphere, and performs additive manufacturing printing after powder spreading, thereby avoiding the problems that a molten pool in the traditional metallurgical process is in a high-temperature state (about 1600 ℃) for a long time, the low-boiling-point easily-oxidizable metal elements are difficult to add in the smelting process, and the steel and the low-boiling-point easily-oxidizable metal are easy to react with oxygen together to generate complex oxidized inclusions to influence the performance of the product.
(2) By the mixed printing process and the mixed printing device for the special steel powder and the low-boiling-point easily-oxidizable metal powder, the harm caused by high oxygen content after the special steel powder is prepared into powder can be counteracted by stably controlling and adding the low-boiling-point easily-oxidizable metal with higher content (more than or equal to 60 ppm). Meanwhile, the low-boiling-point easily-oxidized metal with higher content (more than or equal to 60 ppm) can be added through stable control, so that a final printed product containing a trace amount of low-boiling-point easily-oxidized metal component can be obtained, the problem that the metal is difficult to add in the traditional metallurgy mode is solved, and the possibility is provided for utilizing the low-boiling-point easily-oxidized metal to carry out component design so as to improve the alloy performance.
(3) The special steel powder and low-boiling point easily-oxidized metal powder mixing printing process and device are also suitable for printing of two alloy powders with similar particle sizes and different properties in any mixing proportion, and are wide in application range and strong in universality.
(4) The special steel powder and low-boiling point easily-oxidizable metal powder mixing printing device provided by the invention comprises a structural unit in the pre-storage, transfer and mixing links, supports the printing step, is suitable for mixing two kinds of powder which are easily oxidized by contacting with air to perform 3D printing, and comprises but is not limited to additive manufacturing of mixing printing of low-boiling point easily-oxidizable metal powder and various alloy steels, stainless steels, heat-resistant steels, high-strength steels, high-temperature alloys and other materials.
(5) The special steel powder and low-boiling-point easily-oxidizable metal powder mixed printing process and device provided by the invention can improve the content of low-boiling-point easily-oxidizable metals in additive manufacturing products (such as special steel), reduce oxygen elements in steel, change the existence form of oxide inclusions, reduce the content of the oxide inclusions, reduce the burning loss of alloy elements in the special steel powder printing process, and improve the performance of special steel printed parts.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings, in which like numerals refer to like parts throughout, are for the purpose of illustrating particular embodiments only and are not to be considered limiting of the invention.
FIG. 1 is a process flow chart of the mixed printing of special steel powder and low-boiling point easily-oxidizable metal powder;
FIG. 2 is a schematic view of a part of a printing apparatus for mixing special steel powder and low-boiling point easily-oxidizable metal powder;
FIG. 3 is an oxygen potential diagram of several typical low boiling point easily oxidizable metals;
FIG. 4 is a diagram of a product printed by mixing special steel powder and cerium powder in example 316L.
In the figure, 1-a first powder bin, 2-a second powder bin, 3-a first high-precision adjusting valve, 4-a second high-precision adjusting valve, 5-a powder mixing bin, 6-a powder storage bin, 7-a powder scraping plate and 8-a printing plate.
Detailed Description
The method for adding a low-boiling point easily oxidizable metallic element to a steel product and the printing apparatus will be described in further detail with reference to specific examples, which are provided for purposes of comparison and explanation only, and the present invention is not limited to these examples.
In special steel products, the low-boiling, easily oxidizable metallic elements are generally added during the metallurgical process. In the traditional metallurgical processes such as vacuum metallurgy, electroslag metallurgy and the like, a molten pool is about 1600 ℃ for a long time when special steel is smelted, low-boiling-point easily-oxidizable metal elements are difficult to add in the smelting process, and the low-boiling-point easily-oxidizable metal is easy to react with oxygen to generate complex oxidized inclusions, so that the performance of a product is influenced.
When special steel containing low-boiling-point easily-oxidized metal elements, such as rare earth steel, is prepared by adding rare earth elements in a smelting stage in the prior art and preparing a steel product containing the rare earth elements by adopting an additive manufacturing method, the steel powder containing the rare earth elements is generally obtained by smelting through the traditional metallurgical processes such as vacuum metallurgy, electroslag metallurgy and the like, and then the qualified steel powder for additive manufacturing is obtained by four methods, namely a plasma rotating electrode method (PREP), a plasma atomization method (PA), a GAs atomization method (GA) and a plasma spheroidization method (PS). This method has two problems: (1) After the parent metal (oxygen content is less than or equal to 20 ppm) is prepared into the special steel powder (with the diameter of dozens of microns), the specific surface area of the powder is large, so that the oxygen content of the special steel powder is increased suddenly (the oxygen content is 100-400 ppm) because the powder is easy to adsorb oxygen in the protective atmosphere, and the performance of the product is influenced; (2) In the process of obtaining steel powder by smelting through the traditional processes of vacuum metallurgy, electroslag metallurgy and the like, because a molten pool is about 1600 ℃ for a long time, the smelting process of adding rare earth elements needs to strictly control the processes, such as temperature, reducing atmosphere and the like, and the burning loss is large and the cost is high. In addition, the rare earth content in the final steel is not easy to be stably controlled, and some rare earth exists in the steel in the form of oxide, so that the rare earth cannot play the due effect. In order to solve the technical problems, the invention provides a method for adding low-boiling-point easily-oxidizable metal elements into a steel product.
Specifically, the method for adding the low-boiling point easily-oxidizable metal element into the steel product provided by the invention comprises the following steps:
step 1: respectively screening the steel powder and the low-boiling point easily-oxidized metal powder in granularity under the protective atmosphere and sealing for later use;
specifically, steel powder and low-boiling point easily-oxidizable metal powder are respectively subjected to particle size screening in a powder screening machine which is introduced with argon gas, powder which meets the particle size requirement is selected, and sealed and stored by a sealing bag for later use;
step 2: drying under a protective atmosphere, cooling to room temperature, and then filling into a first powder bin and a second powder bin for later use;
specifically, argon is introduced into a vacuum baking oven for 5-10 min, a sealing bag filled with steel powder and low-boiling-point easily-oxidizable metal powder is opened in an argon environment, the steel powder and the low-boiling-point easily-oxidizable metal powder are flatly laid in different baking trays, the baking is carried out when the vacuum degree is less than or equal to 100Pa, and the steel powder and the low-boiling-point easily-oxidizable metal powder are respectively filled into a first powder bin and a second powder bin through inner wall smooth hoses under the protection of argon for later use after being cooled to room temperature.
And step 3: accurately controlling the weight of steel powder and low-boiling-point easily-oxidized metal powder to be fed into a powder mixing bin;
specifically, the powder bins in the step 2 are respectively connected to the upper part of a powder mixing bin filled with argon through pipeline valves, a high-precision adjusting valve is arranged on a pipeline close to the powder bins, and special steel powder and low-boiling-point easily-oxidizable metal powder in the powder bins are fed into the powder mixing bin (m) by accurately controlling the weight of the special steel powder and the low-boiling-point easily-oxidizable metal powder through the high-precision adjusting valve controlled by a computer program Boiling powder And m Powder under steel )；
And 4, step 4: uniformly mixing the powder;
specifically, the powder falling from the powder bin is uniformly mixed by a mechanical stirring paddle in the powder mixing bin and then enters the powder storage bin.
And 5: powder spreading, and additive manufacturing and printing;
specifically, the mixed powder is flatly laid in a printing disc by using a powder scraping plate of the additive manufacturing printing equipment for additive manufacturing printing, so that the addition of low-boiling-point easily-oxidized metal elements in the steel product is realized.
In order to realize the full utilization of the raw materials, the method also comprises the following steps after the step 5:
step 6: recovering the mixed powder and returning the mixed powder to a powder storage bin;
specifically, after one round of printing is finished, the mixed powder is recovered, collected under the protection of argon atmosphere and returned to a powder storage bin, and the printing is continued;
and 7: after printing is finished, recycling the mixed powder;
specifically, after all printed parts are printed, the residual mixed special steel powder and low-boiling-point easily-oxidized metal powder are recovered, and the special steel base metal is smelted by using the traditional metallurgical process and equipment again.
It should be noted that the steel powder of the invention adopts the traditional metallurgical technology and equipment of converter/electric furnace process, vacuum induction furnace, atmosphere protection electroslag furnace, etc. to prepare the steel base material. Then, the steel base material is prepared into primary steel powder by a plasma rotating electrode method (PREP), a plasma atomization method (PA), an air atomization method (GA) or a plasma spheroidization method (PS).
The low-boiling-point easily-oxidized metal powder is characterized by being easily combined with oxygen to be oxidized or simultaneously has the characteristics of low boiling point and being easily combined with oxygen to be oxidized, and comprises but is not limited to one or more of Mg, ca, ce and La. The thermodynamic characteristics of several typical low-boiling easily-oxidizable metallic elements and their oxides are shown in table 1, and the oxygen potential diagram is shown in fig. 3.
TABLE 1 thermodynamic characteristics of several low-boiling easily oxidizable metallic elements and their oxides
Name of Chinese Chemical formula (II) Density g/cm 3 Melting Point C Boiling point of
Magnesium alloy Mg 1.74 651 1107
Calcium carbonate Ca 1.55 842 1184
Cerium (Ce) Ce 6.9 798 3462
Lanthanum (La) La 6.174 920 3464
Magnesium oxide MgO 3.58 2852 3600
Calcium oxide CaO 3.35 2572 2851
Cerium oxide CeO2 7.13 2397 3500
Lanthanum oxide La2O3 6.51 2315 4200
Specifically, the weight M of the above-mentioned low-boiling point easily oxidizable metal powder Boiling water With the weight M of steel powder Steel A = M mixed powder weight ratio of Boiling water /(M Boiling water +M Steel ) And a is more than 25 times of the oxygen content of the steel powder.
Note that the total weight M of the mixed printing powders is required General assembly ＝M Boiling water +M Steel The weight M of the low-boiling point easily-oxidized metal powder is obtained by estimating the number and the weight of the printing parts manufactured by the additive and the powder residual quantity of an equipment pipeline, a powder storage bin and the like Boiling water Weight M of steel powder Steel 。
Specifically, in the step 1, when the steel powder and the low-boiling point easily-oxidizable metal powder are used in a laser printer, the granularity is 15-53 μm; when the steel powder and the low-boiling point easily-oxidizable metal powder are used in a plasma beam printer, the granularity is selected from 53-105 mu m.
The particle size range of the metal additive manufactured powder is 15-53 μm (fine powder) and 53-105 μm (coarse powder), and in some cases (for example, the intensity of an energy source and the size of a light spot are adjusted or special process requirements are required for a printed product), the particle size range can be widened to 105-150 μm (coarse powder). The particle size distribution of the metal powder can be analyzed by a laser particle size analyzer.
The printer using laser as energy source is suitable for using 15-53 μm powder as consumable material because its focusing spot is fine and easy to melt fine powder, and the powder in this particle size range has good fluidity and easy to be dissolved, and the powder supply mode is layer-by-layer powder spreading; in a printer using a plasma beam as an energy source, a focusing spot is slightly thick, and the printer is more suitable for melting coarse powder, and is suitable for using 53 to 105 μm powder as a consumable material, and the powder supply method is coaxial powder feeding.
In the step 1, steel powder and low-boiling point easily-oxidizable metal powder are respectively subjected to granularity screening and sealed storage in a protective atmosphere for later use. Screening the primary special steel powder in a powder screening machine which is communicated with argon, packaging the steel powder which meets the requirement of the granularity by a sealing bag, weighing and recording the steel powder as m 1 And then standby. And recovering the primary special steel powder which does not meet the printing granularity requirement after screening, and smelting the steel base material by using the traditional metallurgical process and equipment again.
Purchasing vacuum-packaged low-boiling-point easily-oxidizable metal powder, screening the low-boiling-point easily-oxidizable metal powder in a powder screening machine filled with argon, selecting and retaining the low-boiling-point easily-oxidizable metal powder in the particle size range of the steel powder for additive manufacturing, and packaging the low-boiling-point easily-oxidizable metal powder in a sealing bag for later use.
Particularly, when the granularity of the purchased low-boiling-point easily-oxidized metal powder is within the special steel powder printing granularity range, the low-boiling-point easily-oxidized metal powder can be directly dried for later use without screening by a screening machine. When the granularity of the purchased special steel powder or the low-boiling point easily-oxidized metal powder is within the printing granularity range, the special steel powder or the low-boiling point easily-oxidized metal powder can be directly dried for later use without screening by a screening machine.
Considering that the protective gas flow (such as argon flow) can cause powder floating, in order to not affect the powder screening, the argon flow in the powder screening machine is controlled to be 10-300 l/min, and the argon is introduced from a transparent hose with the diameter of 10mm of an argon bottle at the corner of the equipment far away from the powder.
Specifically, when the mixed printing device of the powder bin 6 is stored including the powder bin, the powder mixing bin 5 and the powder that connect gradually, the powder bin, the powder mixing bin 5 and the powder storage bin are devices that can be independent inclosed, and all are provided with gas inlet, and gas inlet can set up the corner on the storehouse body, and gas inlet passes through the hose connection with the protective gas unit, can let in protective atmosphere through gas inlet.
Specifically, in the step 2, the drying temperature is 100-200 ℃, and the baking time is 4-8 h.
It should be noted that, in the step 2, the door of the vacuum baking oven is opened, a layer of tinfoil is laid on the baking tray, the steel powder packaged in a sealing manner is put into the vacuum baking oven, the door of the vacuum baking oven is covered with a transparent soft plastic covering with gloves or a covering with the same function, the air in the vacuum baking oven and the covering is evacuated after 5-10 min of argon gas introduction in the vacuum baking oven, the sealing bag containing the steel powder is opened in an argon gas environment, and the steel powder is laid in the tinfoil on the baking tray.
And taking out the sealed packaging bag, closing the door of the vacuum baking oven and removing the coating. The weight of the sealed bag was weighed and recorded as m 2 To obtain the weight of the steel powderIs m Steel ＝m 1 -m 2 Here m Steel ≥M Steel 。
And closing the argon, closing the door of the vacuum baking oven, vacuumizing to be not higher than 100Pa, and drying to remove the possible residual moisture of the steel powder. And after the baking is finished and the temperature is cooled to the room temperature, the air inlet of the vacuum baking oven is communicated with argon, the vacuum is slowly broken, and the argon is introduced into the vacuum baking oven for 5-10 min again. Filling argon gas between the closed vacuum oven door and the covering for 5-10 min by using a transparent soft plastic covering material with gloves or a covering material with the same function, after exhausting air, opening the vacuum oven door, and under the protection of argon gas, making the steel powder (weight m) Steel ) The first powder bin 1 filled with argon is filled in through a hose with a smooth inner wall, the feeding hole of the first powder bin 1 is closed, and the first powder bin is reserved for later use.
Similarly, the screened low boiling point easily oxidized metal powder (weight m) in sealed package Boiling water ，m Boiling water ≥M Boiling water ) And putting the steel powder into a vacuum baking oven, closing the door of the vacuum baking oven, vacuumizing, drying, removing the possibly residual moisture of the steel powder, and filling the baked low-boiling-point easily-oxidized metal powder into a second powder bin (2) filled with argon for later use.
Specifically, in the step 3, the blanking ratio m of the low-boiling-point easily-oxidized metal powder to the steel powder Boiling powder /m Powder under steel Is approximately equal to M Boiling water /M Steel And is combined with M Boiling water /M Steel The difference between the two is less than or equal to 0.01 percent.
In step 3, the first powder bin 1 and the second powder bin 2 are connected to the powder mixing bin 5 through pipeline valves, and before installation, the powder mixing bin 5 is filled with argon to remove air. The powder passing through the pipeline of the first powder bin 1 is controlled by a high-precision blanking adjusting valve 3 through a computer program to accurately control the blanking weight m of the special steel powder Powder under steel The powder passing through the pipeline of the second powder bin 2 is controlled by a computer program to accurately control the blanking weight m of the low-boiling-point easily oxidized metal powder by a high-precision blanking adjusting valve 4 Boiling powder 。
In step 5, the mixed powder of the steel powder and the low-boiling point easily oxidizable metal powder is irradiated with the laser beam and then melted to form a micro molten pool, and the micro molten pool is rapidly solidified after the irradiation of the laser beam is stopped. Therefore, the micro-melting Chi Zhongdi easy-to-oxidize metal powder with boiling point and oxygen bonding part are separated from the molten pool and partially remain in the molten pool in the printing process.
The low-boiling point easily-oxidizable metal M comprises the following existing forms in the additive manufacturing process (wherein s is a solid, l is a liquid and g is a gas):
(1) the newly spread powder exists in solid state as M(s) Powder Represents;
(2) in the molten bath in the liquid state, with [ M ]](l) Fusion furnace Represents;
(3) in gaseous form in or out of the bath, by [ M](g) Fusion furnace Or [ M](g) Fly away Representing;
(4) in metallic form in the solidified alloy, [ M ]](s) Fixing device Represents;
(5) in the form of oxides, in the molten bath, in MOx(s) Fusion furnace Or MOx (l) Fusion furnace Or MOx (g) Melting Represents;
(6) oxide form in solidified alloy, in MOx(s) Fixing device Represents;
(7) leaving the bath in the form of gaseous oxides, at MOx (g) Fly away Representing;
(8) immediately after leaving the bath in the form of gaseous oxides, the gaseous oxides become solid, in MOx(s) Dust (B) And (4) showing.
The low boiling point easily oxidized metal M is combined with oxygen in the molten pool and remains in the molten pool and solidifies along with the alloy, and the reaction formula is shown as follows: [ M ] A](g/l/s) Powder or melt +x[O](l/g)＝MOx(g) Fusion furnace Or MOx (l) Fusion furnace Or MOx(s) Fusion furnace Oxides which have not migrated to the surface of the molten pool in the molten pool remain in the molten pool, solidify in the alloy as the molten pool solidifies and finally become MOx(s) Fixing device ；
The low boiling point easily oxidized metal M is combined with oxygen and then is gasified and separated from a molten pool at high temperature, and the reaction formula is shown as follows: [ M ] A](g/l/s) Powder or melt +x[O](l/g)＝MOx(g) Fly away Oxides formed on the surface of the bath, at high temperatures (e.g. electron beam, laser, high temperature)Reaching 5000-7000 deg.c to gasify and separate from the molten pool and finally becoming MOx(s) Dust (B) 。
When the low boiling point easily oxidizable metal M cannot be reacted with oxygen, M (g) is added Fusion furnace Or M (l) Fusion furnace Or M(s) Powder Existing in the molten pool or floating in the argon environment after leaving the molten pool, finally forming isolated low boiling point easily oxidized metal (M(s) Fly away ) Or remain in the solidified melt pool (M(s) Fixing device ) Or the mixture is solidified with special steel powder to form solidified mixed powder.
By the process, the low-boiling point easily-oxidizable metal (such as Mg/Ca/rare earth and the like) with strong oxygen potential is added, so that the low-boiling point alloy content in the special steel of the product is increased from less than 50ppm to 100-500 ppm, the oxygen content in the steel is reduced from 50-120 ppm to below 50ppm, the existence form of oxidized inclusions in the steel is changed, the inclusion content is reduced, and the original oxide of the steel alloy element is changed into the oxide of the low-boiling point easily-oxidizable metal. Meanwhile, the alloy element burning loss in the steel powder printing process is reduced, and the performance of a special steel printing piece is improved.
Specifically, the steel powder can be special steel powder, and when the special steel powder and the low-boiling-point easily-oxidizable metal powder are mixed and printed, the special steel powder is used as a steel powder raw material.
As shown in fig. 2, the invention also provides a printing device for mixing steel powder and low-boiling-point easily-oxidized metal powder, which comprises a powder bin, a powder mixing bin 5 and a powder storage bin 6 which are connected in sequence;
the powder bins comprise a plurality of powder bins which are respectively and independently communicated with the powder mixing bin 5 and are used for containing various raw material powder. Exemplarily, the number of the filler bins is 2, and the filler bins are a first filler bin 1 and a second filler bin 2 respectively; the first powder bin 1 and the second powder bin 2 are respectively connected with the powder mixing bin through pipelines.
Specifically, in the invention, the first powder bin 1 is a special steel powder bin, and the second powder bin 2 is a low-boiling point easily-oxidized metal powder bin, such as a metal powder bin of Mg, ca, ce, la and the like. The first powder bin 1 and the second powder bin 2 are respectively connected with the powder mixing bin through a first pipeline and a second pipeline.
In order to accurately control the raw material ratio in the first filler silo 1 and the second filler silo 2, the discharge ports of the first filler silo 1 and the second filler silo 2 are respectively provided with an adjusting valve.
Specifically, the regulating valve adopts a high-precision regulating valve, such as a high-precision electromagnetic regulating valve, and the high-precision regulating valve can realize automatic and precise feeding through computer program control. Illustratively, the discharge hole of the first powder bin 1 is provided with a first high-precision regulating valve 3, and the discharge hole of the second powder bin 2 is provided with a second high-precision regulating valve 4.
Specifically, first high accuracy governing valve 3 and second high accuracy governing valve 4 are respectively through fixing on two pipelines on powder mixing bunker 5, are connected with powder mixing bunker 5 valve, and powder mixing bunker 5 and additive manufacturing printer's powder storage bunker 6 is connected through the valve. Preferably, the pipeline adopts a hose with a smooth inner wall.
Specifically, the first high-precision adjusting valve 3 is arranged on a connecting pipeline of the first powder bin 1 and the powder mixing bin (5) and is close to the first powder bin 1; and the second high-precision regulating valve 4 is arranged on a connecting pipeline of the second powder bin 2 and the powder mixing bin 5 and is close to the second powder bin (2).
In order to realize the homogeneous mixing of raw materials, be equipped with mechanical stirring rake in the powder mixing bunker 5, including the center pin and install in the paddle of center pin, the paddle is the cambered surface paddle, and quantity is 3. The paddle rotates in the whole process until the powder blanking is finished.
In order to reduce the introduction of oxygen and avoid the oxidation of the raw materials, the links of pre-storing, transferring and mixing the raw materials are all carried out under the protection of atmosphere, and the printing device for mixing the steel powder and the low-boiling point easily-oxidized metal powder also comprises a shielding gas unit.
In order to provide protective atmosphere for the first powder bin, the second powder bin and the powder mixing bin, the first powder bin, the second powder bin and the powder mixing bin are all devices which can be independently sealed, and are provided with gas inlets, the gas inlets are connected with a protective gas unit, and the protective atmosphere (such as argon) can be introduced through the gas inlets.
In addition, the process for mixing and printing the steel powder and the low-boiling point easily-oxidized metal powder is suitable for materials such as various alloy steels, stainless steels, heat-resistant steels, high-strength steels, high-temperature alloys and the like, and can also be used for mixing and printing two different alloy powders A and B in any proportion.
Example 1
This example illustrates the preparation of a cerium-containing 316L special steel product.
Designing and printing a plurality of cerium-containing 316L special steel hollowed-out lettering cards with the length of 10cm, the width of 10cm and the height of 10cm, wherein the total weight of special steel powder is about M Steel ＝20kg。
The raw materials comprise:
about 40kg of primary special steel powder (117 ppm of detected oxygen content); 50kg of 316L special steel base material is smelted by a 100kg vacuum induction furnace (the detected oxygen content is 10 ppm), about 40kg of primary special steel powder is prepared by a plasma rotating electrode method (PREP) (the detected oxygen content is 117 ppm), and the primary special steel powder is packaged for standby by a sealing bag.
The components of the primary special steel powder are shown in the table 2 in percentage by mass:
TABLE 2 comparative and examples 316L special steel powder composition/wt.%
C Si Mn Cr Ni Mo O
0.027 0.056 1.8 17.5 12.3 2.4 0.0117
The low boiling point easy oxidation metal powder is 1kg of pure cerium powder purchased for vacuum packaging.
The method for adding the low-boiling-point easily-oxidized metal element cerium into the 316L special steel piece comprises the following steps:
step 1:
(1) Selecting the special steel powder, sieving with a powder sieving machine to obtain qualified special steel powder (30 μm or less and 50 μm or less), packaging with sealed bags to obtain 3 bags, and weighing Steel 31.25kg (m) Steel ＞M Steel ) And then standby.
(2) Purchasing 1kg of vacuum-packaged pure cerium powder with the specification of 400 meshes (about 37 mu m), and screening is not needed in the granularity range of the special steel powder required to be printed at this time. The environment was protected by argon gas from a powder sifter, and about 0.2kg of cerium powder was taken and packaged in a sealed bag, and the weight was weighed to 0.19kg.
Step 2:
(1) Pouring special steel powder (the particle size is less than or equal to 50 μm and less than or equal to 30 μm) packaged in a sealing bag into a baking plate of a vacuum baking oven, flatly paving, closing the door of the vacuum baking oven, vacuumizing to 80Pa, baking for 4 hours at 100 ℃, cooling to room temperature, and then filling into a powder bin 2 filled with argon for later use.
3 sealing bags are weighed, and the total weight is 0.58kg, so that the total weight of the special steel powder filled into the first powder bin 1 is calculated to be 31.25kg-0.58kg =30.67kg.
(2) The chamber door of the vacuum baking chamber is opened, the vacuum baking chamber is put into vacuum packaging cerium powder, the chamber door of the vacuum baking chamber is wrapped by transparent soft plastic wrapping materials with gloves or wrapping materials with the same function, argon is introduced, and the oxygen content detector can be utilized to detect the oxygen content to ensure the argon filling evacuation effect.
After the enclosed space formed by the vacuum baking oven and the coating is completely exhausted, the vacuum packaging bag of the cerium powder is opened without damaging the argon protection environment, the cerium powder is laid in the baking plate, and the door of the vacuum baking oven is closed. The transparent soft plastic covering with the gloves is collected. Vacuumizing to 80Pa, and baking at 150 deg.C for 6 hr.
After cooling to room temperature, the transparent soft plastic coating with gloves is wrapped on the door of the vacuum baking oven, and argon is introduced into the air inlet of the vacuum baking oven to break vacuum. After breaking vacuum, after completely exhausting air from the enclosed space formed by the vacuum baking oven and the coating, the dried cerium powder is filled into a second powder bin 2 filled with argon by using a transparent hose, and the weight m of the low-boiling-point cerium oxide powder is Boiling water And (4) 0.19kg for standby.
Preparing powder for this printing: special steel powder m Steel =30.67kg, low boiling point easy-to-oxidize metal cerium powder m Boiling water 0.19kg, cerium accounts for 0.19/(30.67 + 0.19) =0.616% (more than 50 times of oxygen content 117ppm, namely 0.616% is more than 50 times larger than 0.0117%), and the ratio of the special steel powder to the low-boiling point easily-oxidizable metal powder is 0.19/30.67=0.619%.
And step 3:
the powder storage bin (5) is filled with argon to remove air, then the first powder bin 1 is connected to the powder storage bin 5 through a pipeline with a first high-precision adjusting valve 3, and the second powder bin 2 is connected to the powder storage bin 5 through a pipeline with a second high-precision adjusting valve 4.
The first high-precision regulating valve 3 is controlled by a computer program to realize the accurate control of the blanking weight m of the special steel powder in the powder blanking of the first powder bin 1 Powder under steel =10kg; the blanking amount of the second powder bin 2 at each time is completed by controlling the second high-precision adjusting valve 4 by a computer program, and then the computer program controls the second high-precision adjusting valve to complete the blanking amount according to m Boiling water /m Steel Calculating the blanking weight m of the corresponding low-boiling point easily-oxidized alloy Boiling powder =0.62kg, corresponding to m Boiling powder /m Powder under steel Should be approximately equal to m Boiling water /m Steel ＝M Boiling water /M Steel The error range of the ratio is less than 0.01 percent.
And 4, step 4:
the powder falling from the powder bin 1 and the powder bin 2 is uniformly mixed by a mechanical stirring paddle designed and installed in the powder mixing bin 5, and then enters the powder storage bin 6 for printing.
And 5:
utilize vibration material disk printing apparatus's powder scraping plate 7 to store the storehouse 6 bottoms in the powder and tile the powder that mixes well in print disc 8, carry out vibration material disk and print. The printing main parameters are as follows: the thickness of the powder layer is 30 μm, the scanning interval is 0.15mm, the laser power is 200W, and the corresponding scanning speed is 800mm/s.
Step 6:
after the additive manufacturing completes one round of printing of the printed parts, the recovered mixed powder is collected under the protection of atmosphere and returns to the powder storage bin 6, and additive manufacturing printing is continued.
And 7:
and after all printed parts are printed, recovering the residual mixed special steel powder and the low-boiling-point easy-to-oxidize metal cerium powder, and smelting the special steel base material by using the traditional metallurgical process and equipment again.
Example 1 addition of cerium, a low boiling point easily oxidizable metallic element, in a 316L special steel product, was achieved to obtain a cerium-containing 316L special steel product having an average oxygen content of 34.4ppm, an average cerium content of 134.1ppm, almost all inclusions of cerium oxide, a minimum size of 0.11 μm, a maximum size of 1 μm, and an average size of 0.28 μm. Example part of a printed product see figure 4.
Comparative example
The primary special steel powder of example 1 was used as a raw material, and additive manufacturing printing was directly performed to obtain a product. The chemical composition and oxide case are shown in tables 2 and 3.
Comparative example has an average oxygen content of 91ppm and inclusions of mainly MnO. Cr 2 O 3 Inclusions, minimum size 0.15 μm, maximum size 1.2 μm, average size 0.4 μm.
By adjusting the addition amount of the low-boiling point easily-oxidizable metal element cerium, a 316L special steel product with the cerium content of 100-500 ppm in the product can be obtained, the oxygen content in the steel can be reduced to below 50ppm from 50-120 ppm, the cerium in the steel is all cerium oxide without inclusions, the size of the cerium oxide is 0.1-1 mu m, and the average size is 0.25-0.3 mu m, such as 0.28 mu m.
Therefore, the method realizes the addition of the cerium which is a low-boiling point easily-oxidizable metal element in the 316L special steel product, obtains the cerium-containing 316L special steel product, effectively reduces the oxygen content in the 316L special steel product printed by additive manufacturing, and changes the existence form of inclusions.
TABLE 3 chemical compositions and oxides case wt/ppm of examples and comparative examples
Figure BDA0003291241180000171
Figure BDA0003291241180000181
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (7)

1. A method for adding low-boiling point easily-oxidizable metal elements into a steel product is characterized by comprising the steps of taking steel powder and low-boiling point easily-oxidizable metal powder as raw materials, carrying out particle size screening, drying and powder mixing under a protective atmosphere, and carrying out additive manufacturing printing after powder spreading;
the low-boiling point easily-oxidized metal elements are magnesium, calcium, cerium, lanthanum, zirconium and beryllium;
the powder mixing proportion formula is as follows: a = M Boiling water /（M Boiling water +M Steel ) Wherein a is more than 25 times of the oxygen content in the steel powder, wherein M is Boiling water The weight of the low boiling point easily oxidized metal powder is M Steel Is the weight of the steel powder.
2. The method according to claim 1, wherein the steel powder is obtained by smelting in a metallurgical process and then using the steel powder for additive manufacturing obtained by a plasma rotating electrode method, a plasma atomization method, a gas atomization method or a plasma spheroidization method.
3. The method of claim 1, comprising the steps of:
step 1: respectively screening the steel powder and the low-boiling point easily-oxidized metal powder in granularity under a protective atmosphere and sealing for later use;
step 2: drying the steel powder and the low-boiling point easily-oxidized metal powder under a protective atmosphere, cooling to room temperature, and then filling the steel powder and the low-boiling point easily-oxidized metal powder into a steel powder bin and a low-boiling point easily-oxidized metal powder bin for later use;
and step 3: accurately controlling the weight of the steel powder and the low-boiling-point easily-oxidized metal powder to be fed into the powder mixing bin, wherein the feeding proportion m of the low-boiling-point easily-oxidized metal powder and the steel powder Boiling powder /m Powder under steel And M Boiling water /M Steel The difference is less than or equal to 0.01 percent;
and 4, step 4: uniformly mixing the powder;
and 5: and (4) spreading powder, and performing additive manufacturing printing to realize the addition of low-boiling-point easily-oxidized metal elements in the steel product.
4. The method according to claim 3, wherein in the step 1, when the additive manufacturing printing is performed by using a laser printer, the particle sizes of the steel powder and the low-boiling point easily-oxidized metal powder are 15 to 53 μm; when the additive manufacturing printing is carried out by adopting a plasma beam printer, the granularity of the steel powder and the low-boiling point easily-oxidized metal powder is 53-105 mu m.
5. The method of claim 3, wherein in step 2, the protective atmosphere is argon.
6. The method as claimed in claim 3, wherein in the step 2, argon is introduced into the vacuum baking oven for 5 to 10min, the sealing bag containing the steel powder and the low-boiling-point easily-oxidizable metal powder is opened in an argon environment, the steel powder and the low-boiling-point easily-oxidizable metal powder are flatly laid in different baking trays, and the baking is carried out under the vacuum degree of less than or equal to 100 Pa.
7. The method according to claim 3, wherein in the step 2, the drying temperature is 100-200 ℃ and the drying time is 4-8 h.
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